Process of recovering resinous matter.



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or 101x130;

v Q mzocnss ow coir-mama aosqm'rmn Be itknown that. I,, W1-1.L1Am J. Housn, residi'xg at. Toledo, in the county of Lucas nd-'S f-at fl {)hio have invented certain new and resin, or oleo-resin, will be termed ligneous matter, for the sake of brevity.

Treatment of-tIa-c vegetable fibrous material containing resin to separate it into resmmls matter, ligneous matter, and cellulose.-The--fibrous material is treated according to the ordinary processes tor the manufacture of wood pulp, as,-by a hotal-kali solution. In the process of digestion the resinous matter and the ligneous.matter are so afi'ected by the chemical used that they are liquefied, while thecell-uioseremains 1 -or pulp,

the nesinons matter, and the alkali .solution containing the ligneous matter, and treat the-two latter separately as hereinafter 1 described.

Quid-useful Improvements in Processes of Se emotion of tkeresinous matter, ligneous Recovering ltesinous Matter, of. which the vmatter, and celZuZosc.-In the process of difollowi'ug 1s a specification. gestion "the resinous-matter and ligneous This invention relates to a method of matter are; L' uefied, while the cellulose retreating a mixture of a solution of ligneous mains as a said; I now separate theycell-lumatter with resinous matter liberated lose from the other two major constituents 6;5 cellulose, whereby each is made available for. of the wood, by dmawing oil the liquid or by utilization, 1 g a filtering operation. In this solution the The process involves the liberation of. the ,lligneous matter remains permanently discellulose of vegetable fibrous material con-' solved, while the resinous matter, now in the t-aining resin, by the action of chemical 1 form of an alkali compound, or resinate, solutions upon the material; the reproduo-. .sepaoates mm the solution inthe solid state tion from the (:l-Jbn'llCfl-l solution of the on standing, and ma- ,then: be remov d, I nal resinous matter, or a product of ltS- -.stead'-of se1m.rating tom the insoluble cellufurther manipulation; the production of oil: lose both the; liquefied resinous matter and and ot gas from the ligneous matter; andv hgneousmatter contained; in the solution, I 76 finally recovering the alkali in case the may al| 1ow tho-resinous matter to separate chemical solution is an alkali compound. and solidify while in contact with the celluv Inasmuch as the art to which this invention lose, and then-draw ofl the solirtion'now conrefers 'consi. ts of a number of related and taim'ing practically none of the resin, recovsequen-tial operations, the present invention ering the, resinous matter from the pill as 80 may be best understood from an ex lana' by a, ue'nt washing- Upon st-andin tion of these individual steps. Accor ingly the ,d issolyel ygsimusmattgr i eei i tatel I will proceed in this specification to set a: portionsetfli igt th b t hil a .n forth the separate consecutive steps as actuother ='porstiio,i a;remains on top, and some is ally practiced, beginning with the provisionf held. in suspension. I may separate the 8-5 of theraw material to be treated and endolid resinates on. top by any of the usual with the. recovery of most of the reagent th d th n se a at the emaining solid that has been employed, and explaining plarresinous matter with the cellulose, draw of? ticularly the one of said processes w 0h the solution-containing the ligneous matter, constitutes my present invention. and then recover the resinous matter in con- V geta le fi us mat r l may-be aid t0 tact with the cellulose from. the cellulose by consist substantially of moisture and insoluwa hing, ble cellulose, soluble ligneous substances, and It is .tohe understood that I do not limit inmany cases resin or oleo-resin. In this y elf m;myparticular method of separaspecification all the organic constituents of -tion l e-invention contemplating broadly 5 the fibrous material aside from the cellulose the .sep imration of the resinous matter from other: lion-cellulose 'matter, and of the separa- 'ti miif resinous nutter irom a solution con taiiiingother now-cellulose matter and pulp. Utilization of the resinous matter.- The resinous matter necovered as above described from a solution resulting from an alkali treatment of fibrous material containing resin, is obtained in the form of alkali com- 'pounds 02E resin, cailsled resinates, which I use directly as soap; or which I preferably pumiziy from coloring matter; or I may obtainby treatment of the alkaline resinous m'atterwi h acids, jree resin, which is a very practicallyunaltered a-sa solid. As the next step in the, process separatelthbcellulose,

valuable product. The alkaline resinous allowed to matter I may also-utlli ie for the manufacture of valuable oils by distillm at destructively; in so doingI recover tie alkali combined in it.

Utilization of the vegetable matter other than celhdose or resinous matter.The liquid containing the extracted ligneous matter, and from which the resinous matter has been separated, is now concentrated as in the or 1- nary processes, by evaporating from it-the major part of the water contained. I now subject theresultin concentrated liquid to a destructive distilfation, 'by which means 1 recover from it gas and oils, which are produced by the action of heat alone, and at the same time the alkali which was contained in the liquid remains in the still, and this alkali is urified and prepared for further use by' t e ordinary process of l-ixiviation, etc. If it is desired, the highly concentrated liquid before bein destructively distilled, may be deprived 0% all the water which it contains by a further heating, as in open pans for instance.

Theoil which I obtain from the ligneous matter is a. valuable commercial product, which, among its other uses, is particularly of service as a wood preservative. The gas produced may be utilized to furnish heat for the reaction or for any other desired purpose. "lhe impure alkali remaining in the still may be rendered liquid by heat, and then withdrawn for purification.

The ordinary processes for obtaining cellulose from wood by chemical means are subject to a number of inconveniences and losses; if, for instance, the chemical used for the treatment of the wood iscaustic soda or .a bisulfite, no product of value is obtained except the cellulose; the rest of the wood has heretofore been 'Wasted and the unused and wasted part of the wood, amounting in most cases to at least as much as the total amount of wood pul produced, has either been burned up in t e incineration of the waste liquor in the soda process or has been pollute the streams, when a bisulfite rocess is used. The recovery of the alkali used in the soda or sulfate proc-v esses has been accomplished heretofore by evaporating the spent liquors to a thick syrupy liquid, which was then fed into an incinerating furnace and the organic matter there destroyed; the impure'alkali resulting wasthen leached, causticized and used on subsequent charges. of material. In my process the whole of the fibrous material is utilized to produce valuable products, none of it is converted into noxious gases, and none of itgoes to pollute the streams. -.In

the old method considerable loss of alkali is also experienced, because the flame which plays upon the alkali residue in the process of incinerating carries it as waste up the chimney. I experience practically no loss of the resinous matter the mixture.

the alkali which I. may tillation of the waste liquid residue is con duotedin a retort. v

In the evaporation of the spent liquors h may have been contained in the wood caused considerable difficulty and loss by separating 'as a. scum use; because the dis in the evaporators and preventing or rendermg very diflicult the economical evaporation because of the foaming of the resinous soap. Under my process, the evaporation of the waste-liquor I experience no difliculty from the foaming of resinous matter, because I have already separated it before the evaporation is commenced.

the cause of difliculty, but utilize it.

It is to be understood that many varia-.

tions are possible, as regards the different steps employed, the their inclusion or omission, the material treated, and the reagents used, without departing from the contemplated scope of my invention, and I intend no limitations whatsoever, except such as are appended claims.

I not only remove set forth in the order of their succession,

Having described my invention what I claim as new and desire to secure by Letters Patent is: U

l. The process of treating a solution of ligueous matter associated with resinous K salts, whlch consists in separating such salts from the solution.

2. The process of treating a mixture of a solution of ligneous matter with resinous salts and liberated cellulose, which consists .in separating the resinous salts from the mixture;

3. The process of treating a mixture of a solution of ligneous matter with resinous salts and liberated cellulose, which consists in separating the cellulose from the mixture, and then separating the resinous salts from the residue. 5

4. The process which consists in treating vegetable fibrous material containing resin with a hot pulping solution and then separating the cellulose, resinous salts, and ligneous matter. I

5. The process of treating a mixture of a solution 'of vegetable matter other than cel lulose or resinous matter with resinous salts,

and liberated cellulose, which consists in allowin the resinous salts to separate and solidifiy and then separating such salts from 6. The process of treating a mixture -of a, solution of vegetable matter other than cellulose or resinous matter with resinous salts and liberated cellulose, which consists in separating-the insoluble cellulose from the mixture, then allowing the resinous salts to separate andjsolidify, and then separating such salts from'the residue. i

7. The process of treating a spent pulping solution containing resinous salts and .then precipitating theresinous salts, and

- matter other than cellulose or res-.

inous 'matter'which consists in allowing the ligneous matter, which consists in separating the resinous salts from the solution.

9. The processpf treating a solution of vegetable matter other than cellulose or resinous matter associatedwith resinous salts and liberated cellulose, which (.OllSlStS 1n precipitating the resinous salts, and then separating such salts froinithe resiclue.

10. The process of treating a solution of vegetable matter other than cellulose or, resinous matter'associated with resinous salts andliberated'cellulose, which consists lll sep-' aratiug the insoluble cel'luloset'rom the residue',-then precipitating the resinous salts, and

lthen' se arating such, salts from'the residue. v. '11.

he process of treating a solution of yeget able matter other than cellulose or res- 'lnous matter associated with resinous salts,

which consists in precipitating the resinous salts, andthen separating such saltsfron'i the residue.

vegetable vegetable I2. The recess which consists in treating brous material containing resin withla hot pulping solution, and then sepm rating the resinous salts from the residue 13. The process which consists in treating vegetable fibrous material containing resin with a. hot pulping solution, then so )ara'ting the'solutiongfrom the cellulose, and t en separating the resinous salts from the residue.

14."The recess which consists in treating brous material containing resin with a hot pulping solution, then precipitate ing the resinous salts,. and then separating such salts fromthe residue,

I vegetable 15., The rocess'which consists in treating brous ,material containing resin with a hot pulping solution; then separating the hot solution from the insoluble cellulose,

arating the vremaining resinous salts from the residue, then recoverlng bjv washing.

from thecellulose the resinous'salts removed with the ce1lulose,'and then" separating the resinous'salts frouifthe wa'shings."

, 17. The ofstreating' a spent pulping solution containingresinous salts and ligneous mutter, whi'chconsists in precipitating the-resinous salts, and then sepavrating such salts from the solution.

'18; The process of treating a .spent pulping solution containing resinous salts and ligneous matter,-which consists in prerating such salts from the residue.

t-i imia' the mi uscule;

*pul 'ing so utioncontaining resinousi. salts an' llgneous matter, which-consists impreeipitating the resinous-salts-by coolin and then separating such salts from the so iti zai;

-20. .'l,he' process of treating a spent pulping solutloncontaining resinous salts and. llgllGOUS'lllfl-ttfll, which cons sts in precipitating the-resinous salts by cooling and consequent subsidence, and then separating such salts from the solution. a

2L The process of treating a solution of \-egetahle matter other than cellulose or resinous .inatter associated with resinous salts and liberated cellulose, which consists in n'evipitatin the resinous salts by subsidence, and hen separating such salts from the residue. v

22.- 'lhe process of treating a. solution of vegetable matter other than cellulose or resinous mutterassociated with resinous salts and liberated cellulose, which consists. in scparatin the insoluble cellulose from the residue,-t urn precipitating the resinous salts by subsidence. and then separating such salts from the residue.

23. The pNx-ess of treating a solution of vegetable matter other thau'eellulosc or resinous nuitter associated with resinous salts,

which consists in precipitating the resinous salts by subsidence, and then separating such salts from the residue.

24-. The process of treating a solution of vegetable matter other than cellulose or resinous matter associated with resinous salts and liberated cellulose, which consists in precipitating the resinous salts b and consequent subsidence, and t en sepa- 25.'The process of treating a solution vegetable matter other than cellulose or resinous matter associated with resinous salts and liberated cellulose, which consists in separating the insoluble cellulose from the residue, then precipitating the resinous salts by. cooling and consequent subsidence, and then separating such salts from the residue.

26. The process of treating a solution of vegetable matter other than cellulose or resinous matter associated with resinous salts, which consists in precipitating the resinous salts by cooling and'consequent subsidence,- and then separating such salts from the residue.

27. The processwhich, consists in treating vegetable fibrous material containing resin with a hot pulping solution, then separating the hot solution from the insoluble cellulose,

cooling then allowing the resinous salts to separate and solidify, and then separating such salts from the residue. I

1 28. The processjwhich consists in treating Corrections in Letters Patent No. 931,608.

vegetable fibrous material containing resin with a hot alkaline pulping solution, and then separatin the,cellulose, the resinous salts, and the ligneous matter.

29. The process which consists in treating vegetable fibrous material containing resin with a hot alkaline pulping solution, then so aratin the hot solution from the inso uble ce lulose, then allowing the resinous salts to separate and solidify, and then separatin the resinous salts from the residue.

precipitating the resinous salts by cooling and consequent subsidence, and t rating such salts from the residue.

32. The rocess of treating a spent alkaline pulping solution containing resinous salts and ligneous matter, which consists in separating the resinous salts from the solution.

33. The rocess of treating a spent alkaline pu ping solution containing resilin sepaous salts and ligneous matter, which consists in precipitating the resinous salts, and then separating such salts from the solution.

34. The process of treating a spent alkaline pulping solution containing resinous salts and ligneous matter, which consists in precipitating the resinous salts by subsidence, and then separating such salts from the solution.

The rocess of treating a. spent alkaline pu ping solution containing resinous salts and ligneous matter, which consists in preci itating the resinous salts by cooling, and t en separating such salts from the solution. I

36.'The rocess of treating a spent alkaline pulping solution containing resinous salts and ligneous matter, which consists in precipitating the resinous salts by cooling and consequent subsidence, and then separating such salts from the solution.

37. The rocess of treating a spent alkaline pu ping .solution containing resinous salts and vegetable matter other than cellulose or resinous matter, which consists in allowing the resinous salts to separate and solidify, and then separating such salts from the solution. I p

38 The process of treating a; solution of li neous' matter associated with resinous sfits, which consists in separating the resinous salts from the residue, then purifying such salts and then treating them with an acid.

39. -The rocess which consists in treating vegetable fibrous material containing resin with a hot pulping solution then separating the resinous salts, the cellulose, andthe ligneous matter, then purifying the resin us salts, and then treating them with an aci 40. The process of treating a mixture of a solution of ligneous matter with resinous salts and liberated cellulose, which consists in separating the resinous salts from the mixture, then purifying such salts and then treating them with an acid.

41. The process of treating a' mixture of a solution of ligneous matter with resinous salts and liberated cellulose, which consists in separating the cellulose from the mixture, then separating the resinous salts from the residue, then puri ing such salts, and

then treating them wit an acid.

42. The process of treating a. solution of l gneous matter assoclated with resinous salts, which consists in separating the resinous salts from the residue, and then treating such salts with an acid.

43. The process of treating a mixture of a solution of ligneous matter associated with resinous salts and liberated cellulose, which consists in separating the resinous salts from the residue, and then treating such salts with an acid.

44:. The rocess of treating a mixture of a solution 0 ligneous matter associated with resinous salts and liberated cellulose, which consists in separating the cellulose from the residue, then separating the resinous salts from the residue, and then treating such salts with an acid.

45. The process which consists in treating vegetable fibrous material containing resin with a hot pulping solution, then separating the cellulose, the resinous salts, and the ligneous matter, and then treating the resinous salts with an acid.-

In witness whereof I afiix my signature in the presence of two witnesses.

FRANK J. KENT, IVIAR'IHA BUSCII'ER.

It is hereby certified that in Letters Patent No. 931,608, granted August 17, 1909,

ilpon the application of' William J. Hough, of Toledo, Ohio, for an improvement in Processes of Recovering Resinous Matter, errors appear in the printed specification requiring correction, as follows: In line 97, page 1, the word of should read or, and in line 109, same page, the word resin should read rosin; and that the said Letters Patent should be read with these corrections therein that the same may conform to the record of the case in the Patent Oflice.

Signed and sealed this 5th day of October, A. D., 1909.

[SEAL] c, BILLINGS.

Acting Commaacwrwr of Patents.

Corrections in Letters Patent No. 931,608.

vegetable fibrous material containing resin with a hot alkaline pulping solution, and then separatin the,cellulose, the resinous salts, and the ligneous matter.

29. The process which consists in treating vegetable fibrous material containing resin with a hot alkaline pulping solution, then so aratin the hot solution from the inso uble ce lulose, then allowing the resinous salts to separate and solidify, and then separatin the resinous salts from the residue.

precipitating the resinous salts by cooling and consequent subsidence, and t rating such salts from the residue.

32. The rocess of treating a spent alkaline pulping solution containing resinous salts and ligneous matter, which consists in separating the resinous salts from the solution.

33. The rocess of treating a spent alkaline pu ping solution containing resilin sepaous salts and ligneous matter, which consists in precipitating the resinous salts, and then separating such salts from the solution.

34. The process of treating a spent alkaline pulping solution containing resinous salts and ligneous matter, which consists in precipitating the resinous salts by subsidence, and then separating such salts from the solution.

The rocess of treating a. spent alkaline pu ping solution containing resinous salts and ligneous matter, which consists in preci itating the resinous salts by cooling, and t en separating such salts from the solution. I

36.'The rocess of treating a spent alkaline pulping solution containing resinous salts and ligneous matter, which consists in precipitating the resinous salts by cooling and consequent subsidence, and then separating such salts from the solution.

37. The rocess of treating a spent alkaline pu ping .solution containing resinous salts and vegetable matter other than cellulose or resinous matter, which consists in allowing the resinous salts to separate and solidify, and then separating such salts from the solution. I p

38 The process of treating a; solution of li neous' matter associated with resinous sfits, which consists in separating the resinous salts from the residue, then purifying such salts and then treating them with an acid.

39. -The rocess which consists in treating vegetable fibrous material containing resin with a hot pulping solution then separating the resinous salts, the cellulose, andthe ligneous matter, then purifying the resin us salts, and then treating them with an aci 40. The process of treating a mixture of a solution of ligneous matter with resinous salts and liberated cellulose, which consists in separating the resinous salts from the mixture, then purifying such salts and then treating them with an acid.

41. The process of treating a' mixture of a solution of ligneous matter with resinous salts and liberated cellulose, which consists in separating the cellulose from the mixture, then separating the resinous salts from the residue, then puri ing such salts, and

then treating them wit an acid.

42. The process of treating a. solution of l gneous matter assoclated with resinous salts, which consists in separating the resinous salts from the residue, and then treating such salts with an acid.

43. The process of treating a mixture of a solution of ligneous matter associated with resinous salts and liberated cellulose, which consists in separating the resinous salts from the residue, and then treating such salts with an acid.

44:. The rocess of treating a mixture of a solution 0 ligneous matter associated with resinous salts and liberated cellulose, which consists in separating the cellulose from the residue, then separating the resinous salts from the residue, and then treating such salts with an acid.

45. The process which consists in treating vegetable fibrous material containing resin with a hot pulping solution, then separating the cellulose, the resinous salts, and the ligneous matter, and then treating the resinous salts with an acid.-

In witness whereof I afiix my signature in the presence of two witnesses.

FRANK J. KENT, IVIAR'IHA BUSCII'ER.

It is hereby certified that in Letters Patent No. 931,608, granted August 17, 1909,

ilpon the application of' William J. Hough, of Toledo, Ohio, for an improvement in Processes of Recovering Resinous Matter, errors appear in the printed specification requiring correction, as follows: In line 97, page 1, the word of should read or, and in line 109, same page, the word resin should read rosin; and that the said Letters Patent should be read with these corrections therein that the same may conform to the record of the case in the Patent Oflice.

Signed and sealed this 5th day of October, A. D., 1909.

[SEAL] c, BILLINGS.

Acting Commaacwrwr of Patents.

Corrections In Letters Patent No. 931,608.

It is hereby certified that in Letters Patent No. 931,608, granted August 17, 1909, upon the application of' William J. Hough, of Toledo, Ohio, for an improvement in Processes of Recovering Resinous Matter, errors appear in the printed specification as follows: In line 97, page 1, the word of should read or, resin should read rosin; and that the said ein that the same may requiring correction, and in line 109, same page, the word Letters Patent should be read with these corrections ther conform to the record of the case in the Patent Office.

Signed and sealed this 5th day of October, A. D., 1909.

C. C. BILLIN GS. miuz'orwr of Patents.

[SEAL] Acting 00m 

